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By G. R. Gardner, D. H. Davis

Increasing realization of the importance of dust control, and the recommendations of various agencies, have led the mining industry to become actively concerned with this problem. The background and necessity for adequate dust-suppression measures have been discussed in a number of publications, including those of the U. S. Bureau of Mines, and the use of spray water to reduce dust at the face and on roadways has been recommended. The problem resolves itself into obtaining adequate dust reduction at a reasonable cost. Inasmuch as the term "adequate dust suppression" has never been clearly defined, nor have permissible limits of dustiness (in terms of dust count) been established, it is apparent that any method selected may be required to meet additional demands. Until the industry has been given some indication of permissible limits of dustiness, no permanent solution is possible. Progress will be somewhat handicapped until such information is available. In addition, dust reduction must be obtained without the addition of any excessive moisture to the coal, since consideration must often be given to: I. Quality standards, particularly reduction in heat value. 2. Handling characteristics, particularly in regard to unloading from railroad cars and bins. 3. Application of dry methods of coal cleaning. 4. Necessity for fine screening within specified limits of oversize and undersize. Little detailed information is available as to the advantages and disadvantages of the several methods of water distribution, the location and protection of sprays, operating data on pressure, quantity of water, and so forth, and results obtained. In 1940 an investigation was undertaken to determine and evaluate the principal factors involved. This paper constitutes a progress report on this work and cannot in any way be regarded as complete on any one of the several phases. Classification of Dust Sources The various sources of underground dust may be classified as primary or secondary. A primary source is one associated with appreciable degradation of size, that is, where the greater part of the actual fines capable of becoming air-borne dust are produced. A secondary source may be considered as one in which the greater part of the fines have been produced at some previous operation and are in such condition that they can be dispersed as air-borne dust. These conceptions appear to be of practical significance, as experience indicates that when dust is controlled at the primary sources the importance of secondary sources is minimized. For these reasons, investigations to date have been concerned principally with the primary sources of dust, and this paper is concerned particularly with one of these—namely, undercutting. In accord with the foregoing definitions, the sources to which the following opera-

Jan 1, 1942

By Alan F. Stewart, Douglas R. Piteau, Dennis C. Martin

Three examples of open pits where toppling failure controls the stability and design of the slopes are described. Two examples involve the design of overall slopes in base metal mines. The third example concerns the analysis and design of remedial measures to prevent toppling failure from occurring in a critical slope in a coal mine. The analytical techniques for assessing toppling failure on a rational basis are discussed for the three examples. This includes an assessment of the important parameters which govern the stability for the toppling failure mode. The geological setting and input data for each example are described, as are the important external or limiting factors pertinent to the sites in question. A statistical cumulative technique was used to assess one of the most important input parameters in the two examples involving overall slope design. Both deep-seated toppling failures, involving the entire slope, and shallow bench failures are considered. Results of the stability analyses and their related engineering significance with regard to slope stability and design are discussed. A sensitivity analysis of various parameters is effectively utilized. Design charts are developed and evaluated accordingly. In the example where toppling failure was unavoidable, the rationale for design of stabilization techniques to prevent toppling is discussed.

Jan 1, 1983

By D. J. Carney, R. L. Stephenson

A sampling technique has been developed for procuring a sample of sinter representative of the entire depth of the sintering bed. The sampling method involves the use of an open-bottom metal basket that rides on the grate of the sintering machine and when removed contains a sample of the sintered product. Additional data have been obtained to indicate that the tumbler test is a suitable means of measuring sinter strength. IN the last few years additional sintering facilities have been installed in both the Pittsburgh and the Chicago district of the United States Steel Co. Since the construction of these sintering plants made possible the use of higher percentages of flue-dust sinter in our blast-furnace burdens, it became important to study means of controlling the quality of sinter to obtain optimum results in the blast furnace. For controlling an operating process, it is necessary first to establish standards by which the quality of the product can be judged. For sinter, it appeared that an important property was its strength or its resistance to degradation during transportation and charging into the furnace. Consequently work was undertaken to establish a standard for sinter strength that could be used both for controlling sintering-plant operations and for correlating sinter quality with blast-furnace performance. The first problem in setting up a standard was that of procuring a sample that would be representative of the sinter made under any particular set of conditions at the sintering plant. Since the United States Steel Co. sintering plants discharge the finished sinter either into a large pit or onto a rotary cooler, the sinter becomes inseparably mixed with material sintered 2 hr before or 2 hr afterwards. For this reason the exact identity of the sinter is lost. A sample selected as the cooler is discharged, or as the sinter is removed from the pit, cannot be said to be truly representative of the sinter made at any specific time. Sampling The first attempt to procure a sample that would be representative of a specific sinter mix and of specific operating conditions was made by stopping the Dwight Lloyd sintering machine and removing an entire pallet full of sinter. This method, however, proved very difficult to perform and interfered considerably with the operation of the plant. To overcome this difficulty, a sampling method was devised by technologists at South Works enabling them to secure, without interrupting the sintering operation, a sample of about 1 cu ft of sinter, representative of sinter for the full depth of the sintering bed. The South Works method involves the use of a steel-frame-work basket. A typical basket is shown in Fig. 1. The basket has been used both with and without crossbars along the bottom. As long as the crossbars are in the same direction as the grate bars on the sintering machine they do not interfere with the sintering process. The basket is set on an empty grate of the Dwight Lloyd sintering machine before it passes under the swinging feed spout, see Fig. 2. When the basket is removed after it has travelled the length of the sintering machine, it contains the sample. Just before the basket is removed, the sinter is scored and chipped to facilitate removal of the sample from the sinter bed. A view of the basket after its removal is shown in Fig. 3. Although the sampling method was originally designed for use on a Dwight Lloyd sintering machine, it can also be used on the Greenawalt type of machine. When used on the Greenawalt-type machine, the basket is placed on the sintering grate before the charging car passes over it, and finally it is removed just before the pan is dumped. Testing After a method of obtaining a representative sample of sinter had been developed, the next step was to select a method of measuring its strength. The irregular shape and size of the sinter pieces precluded the use of a simple compression test for determining strength; consequently, the shatter test and tumbler test were investigated. To perform the shatter test, a sample of sinter, approximately 5 lb, is dropped from a hinged-bottom box at a height of 3 ft onto a steel plate. The broken sinter is sieve-analyzed after a specified number of drops. The tumbler test is performed with the use of a standard ASTM coke-tumbling drum. The drum is 3 ft in diam and is equipped with two lifter bars diametrically opposite one another on the inner periphery of the drum. The drum is rotated at a speed of 24 rpm for 200 revolutions, and after tumbling the sample is sieve-analyzed. To express as single numbers the results of sieve analyses after shattering or tumbling, the method suggested by R. E. Powers1 was employed. This method involved plotting the size of the sieve openings on a logarithmic scale and the cumulative per cent larger than each sieve on a probability scale as described by J. B. Austin.' By interpolating from the plotted data, which in most cases approximated

Jan 1, 1954

By E. A. H. Tays, F. A. Schiertz

In 1893 the Anglo-Mexican Mining Company, Limited, purchased the Guadalupe and adjoining mines, and, after opening up the Guadalupe, constructed a 20-stamp mill, which was started in August, 1894. Although the results were extremely profitable (the ore being very rich and carrying much free gold) they were not satisfactory, because the tailings were found to average about $20 per ton in gold. Early in 1895 the late Mr. James E. Mills made for the company a very thorough study of the subject, and decided that the tailings could be treated most advantageously by the cyanide process. In view of this opinion, Mr. Henry R. Batcheller, of Boston, was sent down in the winter of 1895-96 to experiment on a working scale. Mr. Batcheller was successful; and, during 1896-97, built a cyanide-plant with a capacity for treating 1500 tons per month. This was run until May, 1899, when all the sands suitable for the process had been treated. The mill was stopped about the same time for lack of ore; but no tailings from the mill had gone to the dump since October, 1897, as the values they contained after that date were far too low to warrant further treatment. When the cyanide-plant was stopped there still remained on the dump about 16,000 tons of slimes, consisting of about 75 per cent. of clay-slimes and 25 of sand-slimes. The successful treatment of this very unfavorable material is the theme of this paper. Fig. 1 is a view of the hacienda, taken in 1897.

Jan 1, 1902

By R. E. Collins, Paul B. Crawford

Potentiometric model studies have been made of ertically fractured reservoirs. All fractures originated at he well and extended into the reservoir for various distances. Studies were made to determine the areal sweep efficiencies for line-drive patterns. The areal sweep efficiency for the unfractured system studied war 70.6 per cent. It was found that if the vertical fracture war paralIel with the direction of flood, the areal sweep efficiency may be considerably reduced, approaching zero in some instances. If the fracture was at right angles to the direction of flood, the areal sweep efficiency may be greater than that for the unfractured system. The sweep efficiency depends on the length and orientation of the fracture and direction of the flood. It is concluded that considerable effort should be made to determine the nature and direction of fractures before initiating a flooding program. Such information is required if the maximum sweep efficiency is to be obtained and channeling is to be reduced to a minimum. INTRODUCTION The recent development and application of fracturing techniques to petroleum reservoirs has served to focus considerable attention on the effect such fractures may have on secondary oil recoveries. The opinion has been expressed that fracturing may not alter appreciably the water flooding possibilities. Others have thought that channeling may occur and that the creation of fractures may serve to substantially reduce the possibilities of conducting a successful water flood in the reservoir The purpose of this study was to obtain quantitative estimates of the effect of vertical fractures on the areal sweep efficiencies of line-drive flooding patterns. In presenting this work on vertical fractures, it is not to be inferred that the present fracturing techniques result in producing a vertical fracture. The types of fracture which are created are not known with certainty in every case. Some are believed to be horizontal, others inclined along bedding planes, and some data indicate vertical fracturing. Each fracture will probably exert a different influence on the sweep efficiency of the secondary recovery program; consequently each fractured well should perhaps be considered as a separate problem, requiring a careful analysis. Preliminary work on the effect of fractures on producing capacity of a well indicated that for practical purposes many fractures may be treated as having a nearly infinite permeability This assumption appears to be valid in some instances where the permeability of the fracture is only 10 or 100 times greater than the permeability of the matrix. It is known to depend on the type, orientation and length of the fracture. In realization that fractures of only 0.01 in. width have calculated permeabilities near 5,000 darcys, it is believed that many fractures may be considered as of near infinite permeability without incurring serious error. Primarily for this reason this study was made with fracture analogs of very great permeability compared to the matrix. FRACTURED SYSTEM ANALOG The pattern sweep efficiencies reported here were obtained with the aid of a potentiometric model. The application of this type model for solving reservoir problems has been described in the literature.1,2,3 The electrolyte reservoir was 20 in. wide by 30 in. long by approximately % in. deep. The liquid depth was constant, which corresponded to a constant permeability-feet product from the injection to the production well. The electrolyte reservoir was built to correspond to a unit in the line-drive pattern shown in Fig. 1. This figure shows part of an infinite array of wells having alternate rows of fractured and unfractured wells. The area within the dashed rectangle shows the area generally studied in the model. In using the model to represent a fractured system, a thin strip of copper was soldered to the well or wells and the length and orientation of the strip was made to conform to the vertical fracture under consideration.

Jan 1, 1955

By Charles Pack

Extensive progress has been made in the metallurgy of alloys for die castings. Enthusiastic proponents of some alloys are inclined to make extravagant claims for their materials, which may be justified by physical tests on test bars made from the respective alloys but are seldom justified by the results obtained with commercial die castings made from those alloys. Chemical analysis of the test bars and castings fails to determine the cause of these variations, since they are due to other physical factors entering into the commercial production of die castings. In this paper, an attempt will be made to outline some of the factors in commercial die-casting practice to which these variable results may be attributed, in the hope that the manufacturer of die castings, recognizing the importance of these factors, will devote more attention to them in the design and construction of dies and equipment. In 1914,l the author defined die castings as "metal castings made by forcing molten metal, under pressure, into metallic molds or dies." This definition was given in order to differentiate die castings from other molded metal products such as "permanent-mold" castings, L'slush" castings and similar products that are sometimes erroneously termed die castings. The term "die casting" could be interpreted to include all castings made in metal molds or dies; but since this term, like most of our technical nomenclature, has been developed by commercial practice we must look to this practice for its proper definition. The Germans, with their usual devotion to desecriptive names, have adopted the name of sprilzguss (squirt cast) for die castings. Undoubtedly this name is more descriptive of the die-casting process, where the metal is literally squirted into the die and serves to differentiate this process from other metal mold processes, where the metal is poured into the die. In the earlier paper mentioned, the author also emphasized the fact that the definition given for die castings indicated clearly that the satisfactory operation of the process must comprise three factors, all of which must be considered of vital importance to the successful operation of the die-casting process:

Jan 1, 1931

By Horace W. Hindry

This paper presents the ingredients composing a type of oil-base mud that has been successfully used in drilling oil horizons in California, the effect of ingredient concentrations on physical properties, methods of handling at the well and possible advantages of a waterless drilling fluid with excellent plastering properties. INTRODUCTION AN oil-base mud is a rotary drilling fluid in which oil has been substituted for water as the principal liquid ingredient. In recent years such a mud has been developed and used successfully for drilling the oil horizons of wells in various California fields. There are several types of oil-base mud, but only the type that is currently used to any appreciable extent will be considered at this time. The oil-base drilling-mud compositions used by Shell Oil Company, Incorporated have been covered by several patent applications on which patents are expected to issue at an early date. The purpose of this paper is to present data on the fundamental design of the mud; the ingredients used and their specifications; the effect of ingredient concentration on physical properties; the selection of the proper mud; the facilities needed for handling the mud; and a general discussion [oil] drilling with oil-base mud. In view of the early stage of development of oil-base mud, the great number of variables, and the almost unlimited possible combinations of these variables, which in turn require extensive laboratory study, there are certain irregularities and omissions in the data presented here. However, it is believed that sufficient data are at hand to permit a fairly complete analysis of the characteristics of oil-base muds. In view of the excellent plastering properties of oil-base mud when properly proportioned, its use should: (I) minimize the possibility of impairing the natural flow potentialities of the producing horizon such as that resulting from infiltration of water from water-base muds; (2) permit smaller clearances for setting liners, since the mud sheath has no appreciable thickness; (3) eliminate the possibility of clogging the perforations of the liner with thick mud sheath; (4) facilitate the removal of the mud sheath from the walls of the hole, for its mud sheath has no appreciable strength; (5) assist in drilling through formations, such as "heaving shale," where water wetting appears to be a source of difficulty. (6) permit cores to be obtained without contamination from drilling water. FUNDAMENTAL DESIGN OF AN OIL-BASE MUD In the design of any rotary drilling mud it is necessary to select materials that will fulfill the following requirements: (I) act as the liquid medium and regulate the viscosity; (2) impart initial and final plastering properties; (3) give gel strength and structure in order to prevent settling; (4) serve as a weighting material. The

Jan 1, 1941

By James V. Thompson

SINCE it was introduced in 1943 to recover chromite from Oregon beach sands, the Humphreys spiral concentrator has proved successful in several fields of wet mineral beneficiation. By the end of 1957, 9390 Humphreys spirals had been manufactured. Most of these are still in service. The spiral does not offer a panacea for all mineral dressing problems. Its proper application can best be determined by test work. Spirals present a unique advantage for the metallurgist to make tests in a full-size machine rather than a miniature model, without the risk involved in scaling up results. With only 10 to 40 lb of sample, the operator of a closed circuit test unit employing a full-size Humphreys spiral can conduct preliminary tests with full-scale loadings of 0.5 to 2.5 tph. With larger samples, from 300 to 500 lb, he can run longer multi-stage tests to obtain reliable data for the next step-pilot plant design. The manufacturer of the Humphreys spiral concentrator maintains a fully equipped ore dressing laboratory and by insisting on test work prior to sales has largely prevented misapplication of the spiral.

Jan 1, 1958

By Merton C. Flemings, Harold D. Brody

Analyses that include diffusion of solute in the solid phase are formulated to describe solute redistribution in dendritic solidification of metallic alloys. The analyses are based on conditions that include negligible undercooling before nucleation of solid phases, negligible increase of solute in advance of the tips of growing dendrites, complete diffusion within the liquid over distances the order of dendrite spacings, and a plate-like dendrite morphology. The classical nonequilibrium freezing equation, Cs = kCo(I - fS)k-l accurately describes solute redistribution between dendrite arms for the solidification processes considered, provided diffusion in the solid is negligible. To account for the effect of diffusion in the solid, an analytic expression is given which is similar inform to the classical expression. 172 addition, a numerical-analysis procedure is etnployed to examine in more detail the effect of diffusion both during and after solidification. The analyses are intended for application to solidification of castings and ingots to describe a) final solute distribution after solidification and cooling to room temperature (microsegregation) and b) local fraction solid as a function of ternperatcre within the solidifying casting or ingol. SOLUTE redistribution in cellular and dendritic solidification has been discussed quantitatively in recent papers'-3 and in a series of earlier work.4-6 However, none of the analyses developed have permitted close correlation of theory with final solute distribution (microsegregation) observed in castings and ingots. In this paper, discussion is given of approximations which may reasonably be made in mathematical treatment of microsegregation, and analyses are presented based on these approximations. Numerical results are given for Al-Cu alloys. In a second paper the analyses will be compared with exeriment.7 CLASSICAL ANALYSIS The classical quantitative treatment of solute redistribution within a closed "volume element" has been derived repeatedly, for example by Gulliver,4 Scheil,' and Pfann.' This "classical nonequilibrium solidification equation" is written for constant partition ratio: where Cs = interface composition of the solid when the weight-fraction solid within the "volume element" is fs (weight fraction, wt pct); k = equilibrium partition ratio; Co = initial alloy composition within the volume element (weight fraction, wt pct). Assumptions of Eq. [11 are: 1) There is negligible undercooling before nuclea-tion, or from curvature or kinetic effects. 2) There is no mass flow in or out of the volume

Jan 1, 1967

By S. Usui, I. Iwasaki

The adsorption mechanism of dodecylammonium acetate (DAA) on mercury in potassium fluoride solutions at natural, near neutral pH was investigated. Difler-ential capacity combined with electrocapillary measurements on a dropping mercury electrode were found to provide a sensitive and reliable approach. A shift in the electro capillary maximum (or the point-of-zero-charge) towards positive polarization of the surface due to the adsorption of amine indicated a specific affinity of dodecylammonium ion for mercury surfaces. The amine was shown to adsorb competitively with potassium ion on mercury. Through correlation of the adsorption density of the amine, calculated from the thermodynamic analyses of the electrocapillary curves, and of the diflerential capacity curves, the adsorbed state and the orientation of the amine at the interface were considered. The similarities and the differences in the adsorption behavior of the amine on mercury and on such ionic solids as quartz, silver sulfide, and silver iodide were evaluated. With the promise of flotation providing a cheap and large-scale process for the upgrading of low-grade ores and magnetic concentrates, the iron ore industry has made a sustained search over the years for a flotation reagent of general applicability and high selectivity. Having shelves full of commercial reagents already on hand and anticipating more, both the users and the suppliers are in need of an experimental approach sensitive enough to differentiate the individual characteristics in each group of reagents. Therefore, the adsorption behavior of various flotation reagents on mineral surfaces from aqueous solutions has been a subject of much investigation. The current view of adsorption based on the electrical double-layer theory is formulated on the assumption that certain ions in solution act as potential-determining ions. Their concentrations fix the potential drop across the double layer and their adsorptions govern the surface charge.' Two methods used to study the adsorption

Jan 1, 1971

By E. T. Hayes, A. H. Roberson, M. H. Davies

ZIRCONIUM has been produced on a pilot-plant scale for only a few years, but the potential uses have led a large number of research establishments to engage in a thorough study of the metal and its alloys. The work described in this paper is part of a cooperative project between the Bureau of Mines and the Air Materiel Command. The Zr-Cr system was one of the first investigated because of the possibilities of improving the properties at elevated temperatures, the chemical corrosion resistance, and the mechanical properties of zirconium in a manner similar to the enhancement of the properties of titanium by additions of chromium. There is no published work on the Zr-Cr system but from the similarity of the metals involved it was expected that it would be similar to the Zr-Fe' and Ti-Cr' systems. The materials used in this investigation were prepared in the Bureau of Mines laboratory at Albany, Ore. Zirconium was produced by magnesium reduction of zirconium tetrachloride, and a typical analysis is as follows: Fe, 0.06 pct; Ox, 0.08; N?, 0.01; C, 0.02; and other impurities such as Al, Pb, Ni, Ti, and Si less than 0.01 pct each. High purity chromium was prepared by treating crushed electrolytic chromium in a stream of dried and purified hydrogen." The resulting powder contained about 0.01 pct 0 and about 0.1 pct total metallic impurities. All alloys were prepared by arc-melting 50 g briquetted compacts of the desired composition in a Kroll-type" arc furnace using an inert atmosphere. The furnace was evacuated twice and backfilled with helium, which was gettered by melting a center zirconium button immediately before the alloys were melted. Alloys were remelted at least once to insure greater uniformity of composition and subsequently were annealed in vacuum at 1250°C for 48 hr. Fairly homogeneous alloys were obtained by this means; a slight loss of chromium from the surface by evaporation during the high temperature homogenization was noted. All alloys were analyzed for chromium and gave results in good agreement with the nominal composition. Spot checks on tungsten and nitrogen showed pick-up of these elements to be negligible. Over 70 alloys were prepared for use in this investigation; only the critical ones are shown in Table I. Alloys containing up to 10 pct Cr were amenable to hot working at 850°C and a number of these were sheath rolled to 1/16 in. thickness. Specimens were cut from the sheet for use as metallographic samples. For the thermal analysis a differential couple was used in conjunction with an X-Y recorder, the temperature of the specimen and the difference in ternperature between it and the standard nickel body were recorded simultaneously. Heating and cooling rates of 5°C per min were used. The sensitivity of the instrument was such that a difference in temperature between the specimen and standard equivalent to 0.1 mv produced a deflection of 1 in. on the recording chart. The chromel-alumel thermocouples were checked against a Bureau of Standards calibrated thermocouple. Melting-point determinations were made in a high vacuum induction furnace using an optical pyrometer. The pyrometer, calibrated against nickel, copper, and zirconium (iodide process) under near black body conditions, was focused on the base of a hole drilled in cylindrical samples. A North American Philips Geiger counter X-ray spectrometer was used for all diffraction studies. This instrument, in addition to supplying precise intensity measurements of planar reflections, has an added advantage in that metallographic specimens mounted in bakelite can be used directly, and this

Jan 1, 1953

By D. A. Thomas, M. F. Comerford

Poly crystalline wires of Fe-3.2 wt pct Si were cold-drawn to 31, 66, and 87 pct reductions of area. Mechanical properties and tnicrostructures were studied after recovery and re crystallization. An initial increase in strength during recovery was ascribed to strain aging, and subsequent softening was largely due to polygonization rather than re-crystallization. No unique actioation energies could be determined for the recovery process. Rather, activation energies ranged from 60,600 cal per mole at 10 pct recovery to 83,200 cal per mole when recovery was 50 pct complete. Sites for the nucleation of recrystallization were found to depend on time and temperature. In the early stages of re-crystallization, nucleation occurred in deformation hands. Later, or at high temperatures, recrystal-lized grains were nucleated primarily al grain boundaries. Polygonized structures did not seem to be preferred sites for nucleation. MUCH of the research on deformation, recovery, and recrystallization processes in bcc materials has been performed on single crystals or lightly worked polycrystals. Little study has been devoted to the relation of mechanical properties to micro-structure in polycrystals after severe deformation and subsequent annealing. This paper presents the results of a study of the tensile properties and microstructures of Fe-Si wires drawn varying amounts and annealed at a series of temperatures. EXPERIMENTAL PROCEDURE The experiments were carried out on an alloy of the following composition: 3.2 wt pct Si, 0.08 Mn, 0.016 C, 0.005 0, 0.0002 N, 0.0001 H, 0.008 P, 0.034 S. The material was received as l-in.-sq bars cut longitudinally from a hot-rolled slab provided by the Armco Steel Corp. The bars were forged to 3/8-in. rounds, centerless-ground to 0.250 in., and swaged to '0.108 in. All subsequent reductions were performed by room-temperature wire drawing at the rate of 2 in. per min. Each preliminary draft gave approximately 30 pct reduction of area and was followed by a l-hr anneal at 1010°C in dry hydrogen. Three lots of wire were made with ultimate cold reductions of 31, 66, and 87 pct reduc-

Jan 1, 1965

By J. H. M. Thomeer

A method is presented that provides a mathematical description of capillary pressure curves and, probably, of differences in pore geometry of samples. The technique is based on the observation that the location and shape of a capillary pressure curve reflect characteristics of the pore structure of the sample. INTRODUCTION It has been noted1-5 that the observed differences in shape and location of capillary pressure curves reflect some basic properties regarding the pore geometry of the samples. For example, according to basic concepts of capillarity, the following statements can be made regarding the location and shape of a capillary pressure curve.* The location of the curve with respect to the (Vb)pc and PC axes is a measure of the interconnected pore volume and of the cross-sectional area of the pore first entered by mercury, respectively. The shape of the curve depends on the interconnection of the pores and the sorting of the pore sizes. It has been the object of this study to use this information as a starting point in an attempt to find a unique mathematical description of the PC — (Vv)p, relations of different samples. It may be expected that parameters in such a relation can then be used to describe differences in pore geometry of these samples. For a practical description of the PC — (Vb)p, relation, however, it appears desirable to describe each curve (i.e., each sample) by a limited number of parameters so that the curves taken from all samples form a family, each member of which is uniquely determined by one single combination of values of all parameters.

By C. H. Herty

The results of a study of the open-hearth process from the physicochemical viewpoint are given. This study includes experimentation in small laboratory furnaces and in standard 100-ton furnaces. The behavior of manganese, carbon and phosphorus are quantitatively explained. The action of "residual" manganese is discussed with reference to its relation to iron oxide dissolved in the metal. The solubility of CO in steel and its relation to dissolved FeO and carbon is given. The equation for phosphorus elimination has been tested out on a 200-ton furnace and the results are given in the text. The effect of temperature and slag composition on the elimination of metalloids in the basic open-hearth process has been qualitatively understood since the early days of steel making. The quantitative effect has, however, only recently been brought to attention. The effect of slag composition has received more attention than that of temperature, primarily because the range of finishing temperatures in the basic open-hearth process is small compared to the large variations found in the composition of the slag at different periods during the process, and to the variations occurring with the use of raw materials of different degrees of impurity. The effect of slag composition on the elimination of metalloids has been studied by Styril from the thermochemical standpoint. This method is open to serious errors, in that thermochemical data at 2900' F. are very inaccurate and in many cases completely lacking. Feild2 has calculated equilibrium constants from the rate at which the metalloids are eliminated. The effect of slag viscosity on rate of elimination will affect the constants calculated by this method. Whitely,a Colcough4 and others have used slag compositions as the basis for calculation of constants by which the extent of elimination may be calculated.

Jan 1, 1926

By J. D. Hanawalt, C. E. Nelson, J. A. Peloubet

The subject of the salt-water corrosion resistance of magnesium alloys is somewhat like that of the pitting of stainless steels, in that it involves a relatively small. percentage of the applications but receives a much greater proportion of the publicity. Actually magnesium alloys are in use in many exterior applications as well as interior, with no trouble from corrosion. Magnesium and its alloys have a striking stability against atmospheric attack, being far superior to iron. Specimens exposed unprotected to atmospheric weathering for Io Years show only a superficial surface-film formation. The basic nature of magnesium and of its important alloys is that they are also resistant to the attack of salt water even in an unprotected state, giving substantially no loss in weight after one year of alternate immersion in 3 per cent NaCl solution (Fig. 1). This basic behavior is often masked because of the extreme sensitivity of these alloys to certain impurities and combinations of impurities. It is known, and the subject of increasing emphasis, that higher purity leads generally to greater stability for many materials, non-metallic as well as metallic. However, a review of the literature on the corrosion factors in magnesium alloys shows that almost all researchers worked with base metal in which metallic impurities varied in uncontrolled amounts. The major factor, that of metallic impurities, Probably greatly overshadowed the effects of minor ones such as flux inclusions, nonmetallic impurities, porosity, metallographic state, which these researchers presumed to study. In the present investigation the first observation of interest is that whereas magnesium of commercial purity (99.9 per cent pure) has a corrosion rate in alternate immersion in 3 per cent NaCl solution at room temperature of anywhere from 5 to Ioo mg. per sq. cm. per day, the corrosion rate of high.purity magnesium is 0.15 ± 0.05 mg, per sq. cm. per day. The principle followed in the experiments was to add to such base magnesium other elements, singly and in inin in controlled and known amounts and to observe the corrosion behavior of the resulting alloy. These experiments show the existence of what may be called tolerance limits" of magnesium and some of its alloys for certain impurities. The extremely small percentages of impurities involved and the sharpness of the corrosion discontinuities appear to be quite unpredictable, In order to carry on this work, it was necessary to develop an analysis technique suitable to the problem. In some cases it was necessary quantitatively to analyze impurities to less than 0,001 per cent. The experimental data to be presented are based on observation of about 5000 alloy specimens and on more than 50,000 quantitative analyses. while the primary purpose of this paper is to present the experimentally obtained data on corrosion rates as a function of composition, and particularly to demon-

Jan 1, 1942

By J. D. Hanawalt, C. E. Nelson, J. A. Peloubet

The subject of the salt-water corrosion resistance of magnesium alloys is somewhat like that of the pitting of stainless steels, in that it involves a relatively small. percentage of the applications but receives a much greater proportion of the publicity. Actually magnesium alloys are in use in many exterior applications as well as interior, with no trouble from corrosion. Magnesium and its alloys have a striking stability against atmospheric attack, being far superior to iron. Specimens exposed unprotected to atmospheric weathering for Io Years show only a superficial surface-film formation. The basic nature of magnesium and of its important alloys is that they are also resistant to the attack of salt water even in an unprotected state, giving substantially no loss in weight after one year of alternate immersion in 3 per cent NaCl solution (Fig. 1). This basic behavior is often masked because of the extreme sensitivity of these alloys to certain impurities and combinations of impurities. It is known, and the subject of increasing emphasis, that higher purity leads generally to greater stability for many materials, non-metallic as well as metallic. However, a review of the literature on the corrosion factors in magnesium alloys shows that almost all researchers worked with base metal in which metallic impurities varied in uncontrolled amounts. The major factor, that of metallic impurities, Probably greatly overshadowed the effects of minor ones such as flux inclusions, nonmetallic impurities, porosity, metallographic state, which these researchers presumed to study. In the present investigation the first observation of interest is that whereas magnesium of commercial purity (99.9 per cent pure) has a corrosion rate in alternate immersion in 3 per cent NaCl solution at room temperature of anywhere from 5 to Ioo mg. per sq. cm. per day, the corrosion rate of high.purity magnesium is 0.15 ± 0.05 mg, per sq. cm. per day. The principle followed in the experiments was to add to such base magnesium other elements, singly and in inin in controlled and known amounts and to observe the corrosion behavior of the resulting alloy. These experiments show the existence of what may be called tolerance limits" of magnesium and some of its alloys for certain impurities. The extremely small percentages of impurities involved and the sharpness of the corrosion discontinuities appear to be quite unpredictable, In order to carry on this work, it was necessary to develop an analysis technique suitable to the problem. In some cases it was necessary quantitatively to analyze impurities to less than 0,001 per cent. The experimental data to be presented are based on observation of about 5000 alloy specimens and on more than 50,000 quantitative analyses. while the primary purpose of this paper is to present the experimentally obtained data on corrosion rates as a function of composition, and particularly to demon-

Jan 1, 1942

By T. G. Digges, C. L. Vold, M. R. Achter

A study was made of the effect of the growth conditions on the perfection of single crystals of niobium (columbium). Dislocation densities, determined by means of double-crystal diffractometer measurements , were not greatly affected by the method of crystal preparation but could be reduced by annealing treatments. However, the size, sharpness, and tilt angles of the substructures, observed with X-ray reflection macrograph, were sensitive to variations in growth procedures as well as to subsequent thermal treatments. Although the dislocation density was the same in both types, there were more low-angle bound-aries in crystals grown by zone melting than in those prepared by strain anneal. Mechanisms to account for these observations are discussed in terms of dislocation movements. A planned study of the structure-sensitive properties of refractory metals required the use of single crystals of a high degree of structural perfection and, for ease of handling, of large cross section. It appeared that the strain-anneal technique could satisfy both of these requirements. First, crystals grown in the solid state have been reported to be more perfect than those obtained from the melt.' Second, the diameters of rods which may be produced by zone melting should have a theoretical limit determined by specific gravity, thermal conductivity, and surface tension, while the diameter of strain-annealed rods is limited only by practical considerations. Previously it was shown that niobium (columbium) single crystals of 1 in. diam2 may be grown by strain anneal, compared to the 0.5 in. maximum diameter achieved by zone melting, as reported for molybdenum by Belk.3 The current research was undertaken to investigate and optimize the effect of various process variables on the perfection of 1/4 and 1/2-in.-diam niobium single crystals grown by strain annealing and to compare their perfection to those grown by zone melting. Characterization of these crystals was more conveniently accomplished by means of X-ray than by metallo-graphic techniques. EXPERIMENTAL PROCEDURE Specimen Preparation. Zone-melted crystals of 1/4 in. diam were produced by the standard electron-beam zone-melting technique. The swaged and cleaned rods were outgassed, in the solid state at a temperature near its melting point, at a rate of 12 in. per hr, and single crystals were grown by making two molten passes at 2 in. per hr. By maintaining a zone length of 4 to % in., very uniform single crystals several inches long were obtained. For the strain-annealed crystals, an induction heater was used, in preference to other types of heating, to take advantage of the good penetration of large sections. A five-turn coil, 1 in. long, operating at 10 kc and powered by a motor generator, was contained in a vacuum chamber. The rod, suspended from the upper end, was raised through the coil for both recrystallization and crystal growth. In preliminary work single crystals of the same material were also grown with single and multiturn coils powered by a 450-kc generator. A vacuum of 2 X 10-6 Torr was maintained at temperatures up to 2400°C. Starting with electron-beam-melted ingots of 21/2 in. diam, the analysis for which is given in Table I, the material was cold-swaged to the desired cross section of 1/4 and 1/2 in. diam and then recrystallized. The rods were then strained in a tensile machine and converted to single crystals by passing through the induction coil. As with zone melting, control of orientation is possible by the use of special procedures. Other investigators, see for example Williamson and smallman,4 have reported that orientation control may be achieved by a bending technique. In the present work the strained rod is partially lowered through the coil to start the growth of the crystal. Then it is removed and bent at a point in the poly crystalline portion. Finally, it is returned to the chamber and growth is continued "around the corner". This procedure has certain limitations. If the bending operation exceeds the critical strain, recrystallization may take place. Also, the amount of bending which can be imparted to the rod is limited by coil geometry, and up to now has been 10 deg. However, by repeating the bending and growing operations it should be possible to attain any desired orientation. In preparation for X-ray examination, single crystals were sectioned and planed by means of the spark-erosion technique. To obtain the maximum reflected intensity, the (110) plane was exposed for examination. They were then etched 3 to 5 min in a mixture of con-

Jan 1, 1967

By R. Venkateswar, G. C. Sresty

Size measurement is important in characterization of fine particles. Commonly employed size measurement techniques such as sieving, microscopy, and sedimentation are discussed in this paper. Operating principles, advantages and limitations of these techniques are discussed based on the published information and working knowledge with several of these instruments at the authors' laboratories. A brief description of the recently developed equipment for fine particle characterization is also included. At the end of the paper, a rationale is presented for selection of the size analysis equipment based on specific requirements.

Jan 1, 1980

By G. Krauss, J. M. Thompson, H. Y. Kumagai

Boron-doped p-type and arsenic-doped n-type source materials were used to deposit thin silicon films on amorphous fused quartz substrates by cathodic sputtering in argon atmospheres. All as-sputtered films were found to have high electrical resistivities of about 104 ohm-cm, despite controlled variation of the substrate temperature from 50O to 400°C. The high resistivity of the n-type films persisted even after postdeposition heat treatments as high as 1000°C, while p-type films showed a sharp decrease in re-sistivity to values on the order of 1 ohm-cm or lower after heat treatments above 650°C. X-ray and electron diffraction, together with transmission electron microscopy of the p-type films, revealed that the improved electrical properties resulted from two distinct processes. A primary crystallization or recovery within the pains, which were approximately 200Å diam in the as-sputtered films, accompanied the initial sharp drop in resistivity at 650°C. Following this process, a secondary recrystallization or discontinuous grain growth was nucleated in films heated at 1000°C. The resulting significantly increased size of certain grains and the corresponding decrease in grain boundary area accompanied an additional decrease in resistivity after heat treatment at 1000°C. The properties of thin silicon films are of interest because of their possible application in device technology. Although evaporated silicon films on amorphous substrates1-3 and both sputtered and evaporated germanium films4-' have been studied in some detail, sputtered silicon films have not been widely investigated. It has been observed that evaporated silicon films deposited at substrate temperatures below approximately 600°C are amorphous.1,3,9,10 At substrate temperatures higher than this, the films are polycrys-talline, sometimes exhibiting a fiber texture with the fiber axis normal to the substrate surface.' Similar results have been obtained with germanium films, although in this case the substrate temperature for the amorphous to crystalline transformation is reported to be as low as 150OC.5 The mechanism of film deposition by cathodic sputtering differs markedly from that of thermal evaporation. It might be expected, therefore, that the properties of sputtered and evaporated silicon films would also differ. The purpose of our study was to determine the effects of deposition conditions and heat treatments on the electrical resistivity, structure, and composition of thin silicon films sputtered on fused quartz substrates. EXPERIMENTAL DETAILS Apparatus. A schematic diagram of the sputtering apparatus is shown in Fig. 1. The vacuum chamber was enclosed by an 18-in.-diam by 12-in.-high Pyrex bell jar mounted on a stainless-steel base plate. Access holes in the base plate were used to supply argon gas to the chamber, to allow for various electrical feedthroughs, and to provide mechanical motion to the shutter between the source material and substrate. The chamber was evacuated by a pumping system consisting of a 720 liter per sec oil diffusion pump backed by a 13 cu ft per min mechanical pump. Ultimate pressures of less than 1 x 10-6 torr could be achieved. The substrates were securely mounted on the stainless-steel substrate holder by quartz tabs held in place by stainless-steel screws. Temperatures of the substrate holder were measured by a thermocouple inserted within the holder. A quartz lamp was used to heat the holder and temperatures as high as 420°C could be maintained. Deposition Conditions and Procedure. The substrates used were polished fused quartz slides 116 by 1-12 by 3 in. and were outgassed at 200°C for 1 hr at a pressure less than 1 x 10-5 torr before film deposition. This was followed by a presputtering period of 2 hr during which the movable stainless-steel shutter was so positioned that deposition on the substrate was prevented. At a sputtering voltage of 5000 v dc and an argon pressure of 0.03 torr, the cathode cur-

Jan 1, 1967

By C. E. Sims

The carbon-oxygen reaction without doubt is the basic reaction in steelmaking. It is important on several counts: In the first place, carbon is the element that distinguishes steel from iron. It is the principal element controlling properties, and its control is of prime concern. Although the principal objective of the carbon-oxygen reaction is to oxidize excess carbon, the accompanying boil should not be underrated. The mechanical agitation, stirring, and mixing resulting from the boil are so useful in the distribution of heat and in promoting uniformity of composition in the bath that, were it not a natural accompaniment of the carbon-oxygen reaction, it is probable that something would have to be invented to replace it. The open-hearth operation, for example, with the bath heated from above by radiation, would be impracticable without the carbon boil. The electric-arc furnace is somewhat less dependent on it, but every melter knows how much easier it is to gain temperature with minimum damage to refractories during the boil than with a dead bath The motor action of the induced current of the induction furnace makes the carbon boil unnecessary but even there a severe oxidation has been found useful in giving greater freedom from porosity in certain steels. The quantitative aspects of the carbon-oxygen reaction have been given considerable attention by a large number of investigators, and the principles of physical chemistry have played an important part in these studies. Physical chemistry is the science of the mechanics and mathematics of chemical reactions. It is possible to study the mechanisms of reactions in a qualitative manner writhout reference to mathematics and thus obtain valuable concepts as to the manner in which the wheels go around. When it is desired to express quantitative relations in these reactions, however, resort to mathematics is not only convenient but necessary. Mathematics may also be regarded as the shorthand language of physical chemistry. A basic relation whose description requires numerous words may be expressed very simply by a mathematical formula or equation. A good example of this is the equilibrium constant for a chemical reaction. Expressed verbally, it is: When a chemical reaction has reached a condition of equilibrium, the Product of the concentration of the reacting substances on one side of the equation, divided by the product of the concentration of the reacting substances on the other side, gives a quotient that is a constant at constant temperature For the carbon-oxygen reaction C + O ^ CO this is expressed simply as % C X % O -%co where K (from the German Konstant) is the equilibrium constant for the reaction. Although mathematics is such a necessary and useful tool, it is also a potential pitfall. Mathematics in itself is an abstract science, which is not inhibited by consideration of mechanisms or materials.

Jan 1, 1948